WO2009019571A2 - Method of dissolving essential oils in water - Google Patents

Method of dissolving essential oils in water

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Publication number
WO2009019571A2
WO2009019571A2 PCT/IB2008/002045 IB2008002045W WO2009019571A2 WO 2009019571 A2 WO2009019571 A2 WO 2009019571A2 IB 2008002045 W IB2008002045 W IB 2008002045W WO 2009019571 A2 WO2009019571 A2 WO 2009019571A2
Authority
WO
Grant status
Application
Patent type
Prior art keywords
water
granules
characterized
essential oil
mannitol
Prior art date
Application number
PCT/IB2008/002045
Other languages
French (fr)
Other versions
WO2009019571A3 (en )
Inventor
Claude Laruelle
Nacim Taleb
Thierry Breul
Original Assignee
Claude Laruelle
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date

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Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILET PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/534Mentha (mint)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/537Salvia (sage)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/57Magnoliaceae (Magnolia family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/61Myrtaceae (Myrtle family), e.g. teatree or eucalyptus
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/75Rutaceae (Rue family)
    • A61K36/752Citrus, e.g. lime, orange or lemon
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/30Cosmetics or similar toilet preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toilet preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0012Galenical forms characterised by the site of application
    • A61K9/0053Mouth and digestive tract, i.e. intraoral and peroral administration
    • A61K9/0063Periodont
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0087Galenical forms not covered by A61K9/02 - A61K9/7023
    • A61K9/0095Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1617Organic compounds, e.g. phospholipids, fats
    • A61K9/1623Sugars or sugar alcohols, e.g. lactose; Derivatives thereof; Homeopathic globules

Abstract

The invention relates to a method of preparing water-soluble granules containing at least one essential oil that is naturally insoluble or not very soluble in water, and also to the uses of this method and in particular for the preparation of pharmaceutical or aromatherapeutical compositions that are in dry form and that make it possible to extemporaneously produce solutions for mouthwashes or for body hygiene washes.

Description

METHOD OF ESSENTIAL OILS IN WATER SOLUBILIZATION

The invention relates to a water-soluble granular preparation process containing at least one essential oil naturally little or not soluble in water, as well as uses of this method and in particular for the preparation of pharmaceutical compositions or aromatherapeutic being in dry form and to extemporaneously produce solutions for mouthwashes, or personal hygiene bathroom

The solutions for mouthwashes containing essential oils commercially available today as the essential oil of peppermint, tea tree melaleuca, clove, lavender, sage, eucalyptus, anise, or lemon, are hydro-ethanolic solutions which are packaged in glass or plastic bottles of a capacity ranging from 5 to 500 ml, and are inconvenient to use since it is caused to move, given their size and risk of breakage and / or soil in poor closing of the bottle. The result is usually a poor adherence by patients who avoid traveling with their bottle of solutions for mouthwashes.

It would therefore be desirable to allow patients to better follow their treatment to provide them with compositions in dry form, preferably packaged in unit doses, easily transportable and able to give, after dispersion in a suitable volume of water, solutions for mouthwashes.

However, it is most essential oils with antiseptic referred could be used in solutions for mouth baths, are soluble in organic solvents but are not or very little water. Also their dispersion in water leads to the formation of either a cloudy suspension, an unattractive appearance, or a biphasic liquid and wherein the essential oil is not evenly distributed, which may translate by a decrease in therapeutic efficacy or aromatherapy mouthwash. To obtain a satisfactory solubilization of these substances, it is appropriate to use an organic solvent, ethanol being most suitable for edible use. However, for obvious reasons of public health and also of convenience, it is not conceivable to propose compositions for mouth baths to be reconstructed, partially or totally, in ethanol.

Known long effervescent tablets intended to allow the extemporaneous preparation of solutions for mouthwashes. Such tablets are, for example, described in US Patents No. 3,772,431, 3,888,976 and 4,919,918. It is in all cases of consumer products, with more vocation to allow cleaning of the oral cavity and teeth, by an effervescent effect or bubble, a disinfection. Therefore, in these patents, the presence of essential oils, is considered only in a very accessory. It should be noted that U.S. Patent No. 4,919,918 proposes to provide a water-solubilizing substances insoluble or sparingly soluble may be present in the tablets, adding an ionic surfactant lauryl-type, n-lauryl sarcosinate or sodium alkylsulfoacétate, which contributes to the desired foaming effect. Such a foaming effect is, however, undesirable for mouthwashes.

It has also been proposed methods for making water-soluble compounds naturally little or not water soluble.

Thus, patent application FR-A-2649611 provides a method for preparing a therapeutic composition containing acetylsalicylic acid of dissolving the active ingredient in a solvent and then impregnating the solution thus formed a carbohydrate nutritional support then evaporate the solvent to yield the microparticles or microcrystals formations of the active ingredient, the crystal growth is limited by the support matrix.

Moreover, patent application FR-A-2613223 provides a process for preparing a solid dosage form is in the form of water-soluble grains containing Ginkgo biloba. According to this process, this compound is dissolved in a solvent in the presence of a surfactant, then this solution is then mixed with a water soluble carrier which is then subjected to granulation. According to this document, the water soluble carrier may either be selected from sucrose, lactose, mannitol and maltodextrins. However, if these processes can improve the solubility of these particular active ingredients that are acetylsalicylic acid and Ginkgo biloba whatever the nature of the water-soluble medium used, they are not entirely satisfactory when applied to solubilize essential oils. The inventors were, therefore, set a goal to provide a method that allows to make a water-soluble or more essential oils naturally little or not soluble in water, so as to be able to prepare compositions which are in dry form and which, although containing one or more essential oils little or not water soluble, are able to form homogeneous and stable solutions (without any phase shift phenomenon) after dispersion in water.

The inventors were, in addition, set a goal to provide a method which, while having these advantages, is simple to implement and requires no equipment other than those which are conventionally equipped language laboratories.

The invention, therefore, relates to a water-soluble granular preparation process containing at least one essential oil mouthwash or for personal cleansing bath, comprising the successive steps of: a) wet granulation or impregnation mannitol as water-soluble carrier in the form of granules by means of a solvent containing at least one essential oil; and of ; b) drying the granules; characterized in that the solvent is an aqueous solution of a nonionic surfactant. As part of their work, the inventors have in fact found that surprisingly, when subjected mannitol in a wet granulation or impregnation by means of a solvent containing an essential oil naturally little or no soluble water, the oil binds to the mannitol without being denatured and remains bound to the latter when the granules are subsequently dispersed in water. This gives a solution in which the oil is completely dissolved and able to exert its therapeutic effects as though its solubilization was made possible by the very hydrophilic property of the mannitol to which it is linked.

The inventors have not yet identified the nature of the link established between the essential oil and mannitol during granulation.

For cons, the existence of that link could clearly be demonstrated by tests showing that if subjecting a solution obtained by dispersing the granules into water filtrations and extractions, one constantly finds oil essential in the fraction where the mannitol and without any traces of essential oil unrelated to mannitol is detected.

By cons when subjected xylitol or sorbitol to a wet granulation or impregnation by means of a solvent containing the same essential oil, and then the dispersion of the granules obtained in water, shows that the essential oil does not remain completely bound to the latter when the granules are subsequently dispersed in water.

Among the nonionic surfactants, preferably using polysorbate 80 as nonionic surfactant. However, other nonionic surfactants such as other polysorbates or poloxamers, may also be used for implementing the process according to the invention. A true essential oil is a natural product extracted from aromatic plants. The extraction can be made from flowers, leaves, roots or seeds. Two manufacturing processes are mainly used: extraction or steam stripping. Mouthwashes containing essential oils are commonly used in dentistry, namely for the treatment of mouth ulcers, gingivitis, dental neuralgia, sore throat or to fight bad breath.

Among the essential oils suitable for use in mouthwashes of the invention include for example: lemon oil, anise oil, bay oil, bergamot oil, bitter almond, camphor , cedar leaf oil, cinnamon oil, citronella oil, clove oil, eucalyptus oil, lavender oil, mustard oil, peppermint oil, pine oil, pine needle oil, rosemary oil, spearmint oil, sassafras oil, lavender oil, thyme oil, wintergreen oil.

For example, it is commonly accepted that essential oils made from clove, lavender, peppermint, sage and / or eucalyptus cleanse and freshen breath, preserve the vitality of the gums while respecting the oral flora. According to a preferred embodiment of this composition, the essential oil is chosen from the essential oils of peppermint, melaleuca tree in tea, clove, lavender, sage, eucalyptus, anise, or lemon.

More preferably, the essential oil is chosen from the essential oils of peppermint, clove, or lavender. According to the invention, these essential oils can be combined, depending on the desired effect.

The solvent used for the granulation or impregnation of mannitol may comprise, in addition, one or more excipients such as a colorant (amaranth, cochineal red, patent blue V, quinoline yellow ...) selected for its compatibility with the oil used and or any additional oils and to impart a pleasing color to the solution resulting from the dispersion of the granules in water, or any other excipient which is desired to associate with the oil and which has, also, a solubility in low or no water.

According to the invention, the composition may be constituted only by the granules as obtained by the method described above. However, although mannitol is itself a sweetener and helps to give the composition of both sweetness and freshness in the mouth, usually it is preferred to mix the granules with one or more sweeteners such as sodium cyclamate, sodium saccharin, aspartame or ammonium glycérinate, and / or optionally one or more flavors (mint, anise, lemon, raspberry ...) to make it more enjoyable both in taste than her perfume, especially if the essential oil used has very advantageous organoleptic qualities.

According to yet another advantageous embodiment of the process according to the invention, the granulation or impregnation is carried out with a quantity of solvent corresponding to 5 to 60% and preferably 10 to 40% by weight of the weight of mannitol, while the solvent has a content by weight of oil between 0.1 and 50% and preferably between 0.3 and 20%. Thus, after the drying of the granules, the latter advantageously have a ratio by weight between the mannitol and essential oils between 20 and 1500 and preferably between 300 and 1000.

According to the invention, the granulation of the mannitol and the drying of the granules are made, preferably, in a planetary mixer and in a ventilated oven at a temperature varying between 20 and 60 ° C depending on the degree of heat sensitivity of or essential oils used. However, it is also possible to carry out the granulation of the mannitol in a fluidized air bed and to use a drying oven for drying of the granules. This drying may also be carried out using a fluidized air bed.

According to yet another advantageous embodiment of the process according to the invention, the latter comprises, subsequently drying the granules, a calibration operation of these granules, for instance by screening on a grid, this calibration being, preferably, conduit so as to eliminate all the granules having a size greater than 5 mm.

The process just described has many advantages. Indeed, to make water soluble essential oils that naturally are not or little, it offers the possibility to realize, from essential oils to low or zero water solubility, the compositions in dry form and able to form homogeneous and stable solutions after dispersion in water. Moreover, this process is simple to implement and uses only raw materials (mannitol, water, nonionic surfactant) readily available and of a cost compatible with exploitation on an industrial scale. Finally, it requires no special equipment and can be implemented using devices which are conventionally equipped language laboratories, wet granulation and the impregnation in fact being commonly used in the manufacture of drugs proposed capsules and tablets.

In the case where it is desired a pharmaceutical formulation in tablet form, it will carry out a compression step after the drying described above.

In this case, it will be appropriate to add beforehand to this compression step one or more excipients chosen from those conventionally used for the compression of powders or granules as flow agents, fillers and lubricants. The invention relates to the use of a method as defined above for preparing a composition in dry form and able to give extemporaneously a solution for mouthwashes, after dispersion in water.

The invention therefore also relates to a composition in a dry form and can achieve extemporaneously a solution for mouthwashes, by dispersion in water, which is characterized in that it comprises granules of mannitol bound to at least one essential oil.

Furthermore, the composition may be in the form of a powder resulting from the mixing of the granules with the excipient, or in the form of tablets. According to another preferred embodiment of the composition according to the invention, the latter is packaged in unitary doses each corresponding to one mouthwash. More preferably, each unitary dose is packaged in a sealed package to the air and water, such as a bag formed of an aluminum foil lined with a polyethylene film, and whose dimensions are chosen so as to contain once opened, a sufficient volume of water to make a mouthwash, which prevents thus the use of a glass that is not always at hand especially when moving. The composition according to the invention has many advantages. Indeed, it disperses easily in water to form a clear solution, homogeneous and highly palatable, even when it contains an essential oil with very advantageous organoleptic properties. Being in a dry form, it removes the risk of deterioration of essential oils tend to be unstable in solution as is mainly the case of essential oils sensitive to oxidation. In unit dosages, it ensures the use of an active dose at each mouthwash. Finally, by its presentation and its ease of use, it offers the possibility of a mouthwash in any circumstance without having to travel with a bottle likely to break or open inadvertently.

The invention further relates to a solution for mouthwashes, characterized in that it is obtained by dispersing in water a composition as defined above.

The invention will be better understood using the additional description which follows, which refers to the preparation of dry compositions of examples to be used for making extemporaneous solutions for mouthwashes and ability demonstration these compositions to form homogeneous and stable solutions after dispersion in water.

It is obvious, however, that this additional description is given only as illustrations of the invention and not in any way constitute a limitation. The following figures illustrate the invention: Figure 1 shows the particle size distribution before dispersion in water of the composition given in Example 4; 2 shows the particle size distribution after dispersion in water of the composition given in Example 4.

EXAMPLE 1: Preparation for pellets mouthwash essential oil of mint poiyrée

555.0 mg is carried 100,000 sachets each containing a composition in the form of granules having the following formulation - per sachet:

Method of preparation:

Solution A: solubilization of 4.5 kg Polysorbate 80 (Montanox® 80 VG PHA) in 7.0 kg of purified water using a propeller mixer for 30 minutes at 100 revolutions per minutes, solution B: solubilization of 1.5 kg of essential oil of peppermint, colorants (4.0 g E131 patent blue and 150.0 g of quinoline yellow E 104) and 0.3 kg of sodium saccharin in solution A in mixing 10 minutes at 200 rpm using a propeller mixer. - Granulation 49.046 kg of DC mannitol, previously sieved on a grid of .800 mm mesh, in a planetary granulator using Solution B (wetting in 2 minutes at 200 rpm, followed by granulation for 5 minutes 200 rpm)

Drying the grain obtained at 25 ° C in a ventilated oven until a residual humidity lower than 2.00% (measurement of the residual moisture at 70 ° C to constant loss in an infra red scales),

Calibration dry grain on a grid of 0.800 mm mesh width.

Example 2: Granule preparation for mouthwash essential oil of lavender

555.0 mg is carried 100,000 sachets each containing a composition in the form of granules having the following formulation - per sachet:

Method of preparation:

Solution A: solubilization of 4.5 kg Polysorbate 80 (Montanox® 80 VG PHA) in 7.0 kg of purified water using a propeller mixer for 30 minutes at 100 revolutions per minute,

Solution B: 0.5 kg of solubilising essential oil of lavender, colorants (4.0 g E131 patent blue and 150.0 g of quinoline yellow E 104) and 0.3 kg of sodium saccharin in solution A by mixing 10 minutes at 200 rpm using a propeller mixer.

Granulation 50.046 kg of DC mannitol, previously sieved on a grid of .800 mm mesh, in a planetary granulator using Solution B (wetting in 2 minutes at 200 rpm, followed by granulation for 5 minutes at 200 revolutions per minute), - drying of the grain obtained at 25 ° C in a ventilated oven until a residual humidity lower than 2.00% (measurement of the residual moisture to 7O 0 C to constant loss in balance in infra-red), dry grain calibration on a grid of 0.800 mm mesh width.

Example 3: Preparation of pellets for essential oil mouthwash clove

555.0 mg is carried 100,000 sachets each containing a composition in the form of granules having the following formulation - per sachet:

Method of preparation:

Solution A: solubilization of 4.5 kg Polysorbate 80 (Montanox® 80 VG PHA) in 7.0 kg of purified water using a propeller mixer for 30 minutes at 100 revolutions per minute,

Solution B: 1.0 kg solubilization of essential oil of clove, colorants (4.0 g Patent Blue El 31 and 150.0 g of quinoline yellow E 104) and 0.3 kg of sodium saccharin in solution a by mixing 10 minutes at 200 rpm using a propeller mixer.

Granulation 49.546 kg of DC mannitol, previously sieved on a grid of .800 mm mesh, in a planetary granulator using Solution B (wetting in 2 minutes at 200 rpm, followed by granulation for 5 minutes at 200 rpm)

Drying the grain obtained at 25 ° C in a ventilated oven until a residual humidity lower than 2.00% (measurement of the residual moisture at 70 ° C to constant loss in a balance to infra-red), - Size dry grain on a grid of 0.800 mm mesh width.

EXAMPLE 4: Preparation of granules for mouthwashes based on essential oils poiyrée mint, lavender and clove is carried 100,000 sachets each containing 555 mg of a composition being in the form of granules and having the following formulation:

Method of preparation:

Solution A: solubilization of 4.5 kg Polysorbate 80 (Montanox® 80 VG PHA) in 7.0 kg of purified water using a propeller mixer for 30 minutes at 100 revolutions per minute,

Solution B: solubilization of essential oils (1.5 kg of essential oil of peppermint, 0.05 kg essential lavender oil and 0.1 kg of essential oil of clove), colorants (4, 0 g of patent blue El 31 and 150.0 g of quinoline yellow E 104) and 0.3 kg of sodium saccharin in solution a by mixing 10 minutes at 200 rpm using a propeller mixer.

Granulation 48.896 kg of DC mannitol, previously sieved on a grid of .800 mm mesh, in a planetary granulator using Solution B (wetting in 2 minutes at 200 rpm, followed by granulation for 5 minutes at 200 revolutions per minute) Drying grain obtained at 25 ° C in a ventilated oven until a residual humidity lower than 2.00% (measurement of the residual moisture at 70 ° C to constant loss in balance IR)

Calibration dry grain on a grid of .800 mm mesh,

Bagging the resulting blend (555.00 mg unit).

Caractéήsation pharmacotechniques (including visual parameters and flow of the final mixture) The results of the checks during manufacture of the latter composition show that the granulation is homogeneous; the grains are formed and homogeneously staining, absence of phase separation phenomena, and the flow rate of the final mixture is less than 10 seconds.

Analysis of the particle size of the granules by sieving

The particle size of the composition of Example 4 was measured according to the particle size classification by sieving powder method (European Pharmacopoeia 2.9.12 V th edition) which consists essentially in passing the granules through a series of sieves of various sizes, to perform weighing of different particle populations sieved and report the weight percent of each of them relative to the initial composition.

Figure 1 illustrates, in a histogram of particle size distribution obtained for the sample and the following table summarizes the particle size values.

The above results show obtaining small granules whose diameter is less than 1 mm.

Analysis of the particle size of the granules by Laser diffraction granulometer

Was performed an analysis of the particle size of the composition of Example 4 by means of a laser diffraction granulometer (red He-Ne laser of 2 mW minimum of 18 mm in diameter and 633 nm length of wave) Mastersizer

Bench Long (Company Malvern Instruments Ltd.) and an MS sampler 1 of the Company is provided in Figure 2.

2 shows that the composition of Example 4 presents results that confirm those obtained by sieving according to the method described above. No measured particle has an average diameter greater than 1 mm, and the median value of the measured particle size is between 300 and 400 micrometers.

Visual analysis of the composition of Example 4 after dispersion samples were prepared by dispersing the contents of a packet - either

555 mg of compositions provided in Examples 1, 2, 3 and 4 in 20 ml of water and a visual analysis of the dispersion obtained concluded to the absence of particles in solution, thus revealing the formation of a true solution essential oils obtained by this process in water.

Claims

1. A process for preparing water-soluble granules containing at least one essential oil mouthwash or for personal cleansing bath, comprising the successive steps of: a) wet granulation or impregnation of mannitol as water-soluble carrier in the form of granulated using a solvent containing at least one essential oil, and; b) drying the granules, characterized in that the solvent is an aqueous solution of a nonionic surfactant.
2. Method according to claim 2, characterized in that the nonionic surfactant is a polysorbate or a poloxamer.
3. A method according to any one of the preceding claims, characterized in that the essential oil is chosen from essential oil of peppermint, tea tree Melaleuca, clove, lavender, sage, d eucalyptus, anise, or lemon.
4. A method according to any one of the preceding claims, characterized in that the granulation or impregnation of mannitol is carried out with a quantity of solvent corresponding to 5 to 60% and preferably 10 to 40% by weight of mannitol.
5. A method according to any one of the preceding claims, characterized in that it comprises, subsequently drying the granules, a calibration operation of these granules.
6. A method of oral tablet preparation containing at least one essential oil mouthwash or for personal hygiene bath, characterized in that it comprises the successive steps of: a) obtaining water-soluble granules previously obtained according to preceding claim; b) adding one or more excipients selected from those conventionally used for the compression of powders or granules as flow agents, filling agents, lubricating agents, flavorings and sweeteners; c) compression of the powder or granules obtained according to step b).
7. A composition which is in a dry form to achieve a solution extemporaneously by dispersing in water, characterized in that it comprises granules formed from mannitol bound to at least one essential oil, said granules being prepared by a process according to any one of claims 1 to 5.
8. Composition according to claim 7, characterized in that the composition is packaged in unitary doses each corresponding to one mouthwash or a personal hygiene bath.
9. A composition according to claim 8, characterized in that each unitary dose is packaged in a sealed package to water and air, and whose dimensions are chosen so as to be able contain, once opened, a volume of sufficient water to make a mouthwash.
PCT/IB2008/002045 2007-08-06 2008-07-29 Method of dissolving essential oils in water WO2009019571A3 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
FR0705777A FR2919802B1 (en) 2007-08-06 2007-08-06 Process for solubilizing essential oils in water
FR07/05777 2007-08-06

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Cited By (4)

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US9173826B2 (en) 2010-02-16 2015-11-03 The Procter & Gamble Company Porous, dissolvable solid substrate and surface resident coating comprising a zync pyrithione
US9233055B2 (en) 2012-10-12 2016-01-12 The Procter & Gamble Company Personal care composition in the form of a dissolvable article
US9295859B2 (en) 2009-12-08 2016-03-29 The Procter & Gamble Company Porous, dissolvable solid substrate and surface resident coating comprising matrix microspheres
US9545364B2 (en) 2010-07-02 2017-01-17 The Procter & Gamble Company Dissolvable fibrous web structure article comprising active agents

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US20040077609A1 (en) * 2001-01-16 2004-04-22 Michael Rubin Oral composition containing NSAIDs and essential oils
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US9295859B2 (en) 2009-12-08 2016-03-29 The Procter & Gamble Company Porous, dissolvable solid substrate and surface resident coating comprising matrix microspheres
US9173826B2 (en) 2010-02-16 2015-11-03 The Procter & Gamble Company Porous, dissolvable solid substrate and surface resident coating comprising a zync pyrithione
US9545364B2 (en) 2010-07-02 2017-01-17 The Procter & Gamble Company Dissolvable fibrous web structure article comprising active agents
US9233055B2 (en) 2012-10-12 2016-01-12 The Procter & Gamble Company Personal care composition in the form of a dissolvable article

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FR2919802A1 (en) 2009-02-13 application
WO2009019571A3 (en) 2009-09-11 application

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